盐析辅助液液萃取结合气相色谱-质谱法测定酱油中4种氯丙醇  

Determination of 4 kinds of chloropropanols in soy sauce by salting-out assisted liquid-liquid extraction combined with gas chromatography-mass spectrometry

作　　者：曾坤 王东旭 王新财 谷贵章 ZENG Kun;WANG Dong-Xu;WANG Xin-Cai;GU Gui-Zhang(Huzhou Institute for Food and Drug Control,Huzhou 313000,China)

机构地区：[1]湖州市食品药品检验研究院,湖州313000

出　　处：《食品安全质量检测学报》2024年第11期182-188,共7页Journal of Food Safety and Quality

基　　金：浙江省市场监督管理局科技计划项目(20200124);浙江省基础公益研究计划项目(LGN21C020001);湖州市科技局公益性应用研究项目(2021GZ29)。

摘　　要：目的建立盐析辅助液液萃取结合气相色谱-质谱法测定酱油中1,3-二氯-2-丙醇、2,3-二氯-1-丙醇、3-氯-1,2-丙二醇和2-氯-1,3-丙二醇的分析方法。方法以D5-3-氯-1,2-丙二醇为内标物,酱油样品经乙腈提取,氯化钠盐析分层,七氟丁酰基咪唑衍生,HP-5MS毛细管柱(30 m×0.25 mm,0.25μm)分离,采用气相色谱-质谱法的选择离子监测模式进行测定。实验考察了盐析助剂、萃取溶剂对4种氯丙醇萃取效率的影响。结果最优实验条件下,4种氯丙醇在0.006~0.120 mg/kg范围内线性关系良好,且相关系数都大于0.999,检出限为0.002 mg/kg,定量限为0.006 mg/kg。在0.02、0.05、0.10 mg/kg的加标水平下,4种氯丙醇的加标回收率为70.2%~103.5%,相对标准偏差为1.6%~5.5%。结论本方法快速、简便、节省溶剂,适用于酱油中氯丙醇的快速定性、定量分析。Objective To establish a method for the determination of 1,3-dichloro-2-propanol,2,3-dichloro-1-propanol,3-chloro-1,2-propanediol and 2-chloro-1,3-propanediol in soy sauce based on salting-out assisted liquid-liquid extraction coupled with gas chromatography-mass spectrometry.Methods Using 3-chloro-1,2-propanediol-d5 as deuterated internal standard,the soy sauce sample was extracted with acetonitrile,salted out by sodium chloride,derived using 1-(heptafluorobutyryl)imidazole,separated by HP-5MS capillary column(30 m×0.25 mm,0.25μm)and determined by gas chromatography-mass spectrometry in selected ion monitoring mode.The effects of salting-out aid and extraction solvent on extraction efficiency of the 4 kinds of chloropropanols were investigated.Results Under the optimal experimental conditions,the 4 kinds of chloropropanols showed good linearity in the range of 0.006–0.120 mg/kg,and the correlation coefficients were all above 0.999,and the limits of detection of the 4 kinds of chloropropanols were 0.002 mg/kg,and the limits of quantitation were 0.006 mg/kg.The recoveries of the 4 kinds of chloropropanols were in the range of 70.2%–103.5%,and the relative standard deviations were in the range of 1.6%–5.5%at the spiked levels of 0.02,0.05 and 0.10 mg/kg.Conclusion This method can provide a good specificity for the rapid qualitative and quantitative analysis of chloropropanols in soy sauce with the advantage of rapid,simple and solvent saving.

关 键 词：酱油 氯丙醇 盐析辅助液液萃取 气相色谱-质谱法 

分 类 号：O657.63[理学—分析化学] TS264.21[理学—化学]